Improvements in pentosan polysulfate sodium quality assurance using fingerprint electropherograms.

Complex samples from polymer production, plant extracts or biotechnology mixtures can be characterized by fingerprints. Currently, the standard approach for sample characterization employs near-infrared (NIR) spectroscopy fingerprinting. Up to now, however, fingerprints obtained by chromatography or electrophoresis could only be visually evaluated. This type of inspection is very labor-intensive and difficult to validate. In order to transfer the use of fingerprints from spectroscopy to electrophoresis, spectra-like properties must be obtained through a complete alignment of the electropherograms. This has been achieved by interpolation and wavelet filtering of the baseline signal in the present work. The resulting data have been classified by several algorithms. The methods under survey include self-organizing maps (SOMs), artificial neural networks (ANNs), soft independent modeling of class analogy (SIMCA) and k-nearest neighbors (KNNs). In order to test the performance of this combined approach in practice, it was applied to the quality assurance of pentosan polysulfate (PPS). A recently developed capillary electrophoresis (CE) method using indirect UV detection was employed in these studies [1]. All algorithms were well capable of classifying the examined PPS test batches. Even minor variations in the PPS composition, not perceptible by visual inspection, could be automatically detected. The whole method has been validated by classifying various (n = 400) unknown PPS quality assurance samples, which have been correctly identified without exception.

Quality control of pentosane polysulfate by capillary zone electrophoresis using indirect detection.

Pentosane polysulfate sodium salt (PPS) is a mixture of multiply charged anionic polysaccharides, used for urological treatment. Several constituents of the polysaccharide can be characterized by a highly reproducible fingerprint. In comparison with earlier approaches the separation efficiency has been further improved using an anionic benzene-1,2,4-tricarboxylic acid buffer (8.7 mmol l-1, pH = 4.9) with indirect UV detection (lambda = 217 nm) and a special capillary pretreatment (1 M NaOH for 10 h at 25 degrees C applying -20 kV). The method has been optimized with regard to buffer concentration and pH. The robustness was tested on several capillaries. PPS was separated from all major synthetic impurities such a sulfate, chloride and acetate. Twelve PPS batches from two manufactures were measured and compared.

[Conformationally restricted pethidine analogs. 5. Synthesis and pharmacologic testing of cis-B-10b-acyl-1,2,3,4,4a,5,6,10b- octahydrobenzo(f)isoquinolines]. / Pethidin-Analoga mit eingeschränkter Konformationsbeweglichkeit. 5. Mitteilung: Synthese und pharmacokologische Prüfung von cis-B-10b-Acyl-1,2,3,4,4a,5,6,10b-octahydrobenzo[f]ischinolinen.

Cyanophenylcyclobuten (1a) gave the corresponding cis-B-configurated 10b-acyloctahydrobenzo[f] isoquinolines 3a-f by Grignard reaction. Cis-B-3b was demethylated to yield the secondary base 3g, which in turn was realkylated to the homologous allyl- and isopentenyl derivatives 3h and 3i. In the writing test the desoxyketobemidon analogon cis-B-3b exhibits a remarkable activity, whereas 3a, c-e are somewhat weaker and 3h and 3i are inactive.